CN105639657A - Method for extracting mineral elements in boxthorn leaves through enzymolysis - Google Patents
Method for extracting mineral elements in boxthorn leaves through enzymolysis Download PDFInfo
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- CN105639657A CN105639657A CN201610074800.7A CN201610074800A CN105639657A CN 105639657 A CN105639657 A CN 105639657A CN 201610074800 A CN201610074800 A CN 201610074800A CN 105639657 A CN105639657 A CN 105639657A
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- folium lycii
- extraction
- enzymolysis
- ultrasonic extraction
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- 239000002366 mineral element Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 26
- 244000241838 Lycium barbarum Species 0.000 title abstract 8
- 235000015459 Lycium barbarum Nutrition 0.000 title abstract 8
- 235000015463 Lycium carolinianum Nutrition 0.000 title abstract 8
- 239000008367 deionised water Substances 0.000 claims abstract description 44
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000000843 powder Substances 0.000 claims abstract description 37
- 238000000605 extraction Methods 0.000 claims abstract description 34
- 238000003756 stirring Methods 0.000 claims abstract description 28
- 108010059892 Cellulase Proteins 0.000 claims abstract description 25
- 229940106157 cellulase Drugs 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000012216 screening Methods 0.000 claims abstract description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 88
- 239000006228 supernatant Substances 0.000 claims description 88
- 238000002137 ultrasound extraction Methods 0.000 claims description 71
- 238000001914 filtration Methods 0.000 claims description 66
- 229960000583 acetic acid Drugs 0.000 claims description 44
- 239000012362 glacial acetic acid Substances 0.000 claims description 44
- 239000007788 liquid Substances 0.000 claims description 24
- 239000000284 extract Substances 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 238000005292 vacuum distillation Methods 0.000 claims description 2
- 108090000790 Enzymes Proteins 0.000 abstract description 6
- 102000004190 Enzymes Human genes 0.000 abstract description 6
- 229940088598 enzyme Drugs 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000005238 degreasing Methods 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 238000000967 suction filtration Methods 0.000 abstract 1
- 239000000706 filtrate Substances 0.000 description 40
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 24
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 24
- 239000011575 calcium Substances 0.000 description 24
- 229910052791 calcium Inorganic materials 0.000 description 24
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 23
- 239000011701 zinc Substances 0.000 description 23
- 229910052725 zinc Inorganic materials 0.000 description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 20
- 229960000935 dehydrated alcohol Drugs 0.000 description 20
- 239000012065 filter cake Substances 0.000 description 20
- 239000002244 precipitate Substances 0.000 description 20
- 230000000694 effects Effects 0.000 description 4
- 229920002678 cellulose Polymers 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- 235000013399 edible fruits Nutrition 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 2
- 235000013373 food additive Nutrition 0.000 description 2
- 239000002778 food additive Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011573 trace mineral Substances 0.000 description 2
- 235000013619 trace mineral Nutrition 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- 206010013486 Distractibility Diseases 0.000 description 1
- 206010058314 Dysplasia Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 102000001554 Hemoglobins Human genes 0.000 description 1
- 108010054147 Hemoglobins Proteins 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 244000241872 Lycium chinense Species 0.000 description 1
- 235000015468 Lycium chinense Nutrition 0.000 description 1
- 208000001132 Osteoporosis Diseases 0.000 description 1
- 241000208292 Solanaceae Species 0.000 description 1
- 208000007502 anemia Diseases 0.000 description 1
- 238000004380 ashing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 235000015872 dietary supplement Nutrition 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 210000004209 hair Anatomy 0.000 description 1
- -1 have that short Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 229920001542 oligosaccharide Polymers 0.000 description 1
- 150000002482 oligosaccharides Chemical class 0.000 description 1
- 108010048734 sclerotin Proteins 0.000 description 1
- 230000035922 thirst Effects 0.000 description 1
- 239000005418 vegetable material Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to a method for extracting mineral elements in boxthorn leaves through enzymolysis. The method is characterized by comprising the steps that 1, raw materials are prepared, wherein the boxthorn leaves are dried; 2, smashing is performed, wherein the dried boxthorn leaves are smashed; 3, screening is performed, wherein boxthorn leaf powder obtained after smashing passes through a 60-80 mesh screen; 4, degreasing is performed, wherein No. 6 light petrol is added to the obtained powder for soaking, stirring is performed, suction filtration and drying are performed, and then the boxthorn leaf powder without fat is obtained; 5, enzymolysis is performed, wherein the obtained boxthorn leaf powder is taken, deionized water is added according to the ratio of 1 g of boxthorn leaf powder / 10-20 mL of deionized water, cellulase is added according to the ratio of 130-150 micro/mL, and stirring is performed for 1-2 hours. On the basis of an existing mineral element process, an ultrasonic wave and enzyme combined extraction method is used for effectively increasing the yield of the mineral elements, so that the raw materials are saved, and production cost is reduced.
Description
Technical field
A kind of method that the present invention relates to enzymolysis and extraction Folium Lycii mineral element.
Background technology
Fructus Lycii (LyciumChinensemiller) is the perennial machaka of Solanaceae, has important using value in medicine, field of food. Traditional medicinal part of Fructus Lycii is fruit and Fructus Lycii, has long value of exploiting and utilizing. Except fruit, blade, tender stem etc. also have significantly high medicinal health care function. Folium Lycii is referred to as " sky essence grass ", cool in nature, sweet in the mouth, and having quenches one's thirst promotes the production of body fluid, and yin nourishing such as is relieved inflammation or internal heat at the effect. Folium Lycii is rich in various trace elements, and its Mineral Elements Content is even more than Chinese wolfberry fruit. Human body is had much important effect by mineral element, when human body lacks, can produce disease. Calcium, ferrum, zinc are all the trace element of needed by human. Ferrum is the requisite material of synthetic hemoglobin, and human body lacks ferrum can cause anemia; The shortage of zinc can cause dysplasia, withered and yellowish hairs, distractibility; Calcium can promote that bone and sclerotin are strong, calcium lack the growth of major effect skeleton and structure, show as osteoporosis. Epidemiological study shows, the mineral element that Chinese residents is easier to lack mainly has the elements such as calcium, ferrum, zinc. People mainly absorb some mineral elements necessary to health from food.
The extracting method of plant Mineral Elements is only limitted to ashing method and nitrification process, and the purpose of extraction is intended merely to its content of detection, and after extracting, these mineral elements have been out edibility, and the extraction of mineral element is destructive by these methods.
Summary of the invention
It is an object of the invention to provide a kind of method that ultrasound wave and enzyme can be utilized to combine and non-destructively extract mineral element contained in Folium Lycii, it is therefore an objective to the mineral element making extraction can as nutrient health supplement or food additive.
A kind of method of enzymolysis and extraction Folium Lycii mineral element, it is particular in that, comprises the steps:
(1) raw material: Folium Lycii is dried;
(2) pulverize: the Folium Lycii after drying is pulverized;
(3) screening: the Folium Lycii powder after pulverizing is crossed 60-80 mesh sieve;
(4) defat: add No. 6 light gasoline in the powder obtained and soak, then stir, then sucking filtration drying, obtain removing the Folium Lycii powder of fat;
(5) enzymolysis: obtain the Folium Lycii powder arrived, add deionized water according to 1g Folium Lycii powder/10-20mL, adds cellulase according still further to 130-150u/mL, stirs 1-2 hour;
(6) acidifying: the sample after enzymolysis is added according to 1g sample/1.5-2mL glacial acetic acid or glacial acetic acid solution, stirs 0.5-1 hour;
(7) ultrasonic extraction: at 30-70 DEG C, ultrasonic extraction 5-25min when 50-100MHz, take the supernatant after ultrasonic Treatment, to precipitate according still further to condition ultrasonic extraction same as before, take the supernatant after ultrasonic Treatment, to precipitate according still further to condition ultrasonic extraction same as before, take the supernatant after ultrasonic Treatment, finally merge the supernatant extracted three times;
(8) filter: the extracting solution sucking filtration that will obtain, discard filtering residue;
(9) concentration: carry out the concentrating under reduced pressure 1/3-1/5 to original volume with the vacuum distillation apparatus extracting solution to obtaining;
(10) dry: by the liquid drying after concentration to mineral element extract.
Step (1) is dried and refers to 50-60 DEG C of drying 8-12h in blast drier.
Step (4) controls No. 6 light gasoline liquid levels and did not have powder 1-1.5cm, control mixing time 1-2 hour.
Step (10) is dried and refers to drying at 50-60 DEG C.
The present invention is on the basis of existing mineral element technique, using the extracting method that ultrasound wave is combined with enzyme, the effective yield improving mineral element, thus having saved raw material, reducing production cost. The inventive method also resides in relative to existing technological merit: (1) provides the method for a kind of efficient and nondestructive extraction mineral element, what utilize is on the basis of acidolysis and the condition of ultrasonic extraction, combine with cellulase, mineral element dissolution rate from Folium Lycii cell and dissolution rate are all increased, thus reaching to save raw material and the purpose of time. (2) advantage that ultrasonic extraction has efficiently, economy, cost are low, saves the cost because labour brings, and once can extract multiple mineral element simultaneously. (5) cellulase hydrolysis cellulose has high efficiency, cellulose hydrolysis can become monosaccharide and oligosaccharide, thus the mineral element that a part is fettered by cellulose is released in hydrolytic process, thus improve extraction ratio. (6) utilizing enzyme process to extract the mineral element that obtains from vegetable material can as edible supplementary or food additive for food processing. (6) equipment used by this method is relatively simple, has simply used pulverizer, ultrasonic device, vacuum pump and vacuum dryer, and therefore its operating cost is relatively low, is more suitable for industrialized production. In sum, enzyme process is a kind of method of high efficiency extraction Folium Lycii mineral element, have that short, mineral element yield consuming time is high, mineral element destructiveness is little, save material and the advantage such as operating cost is low, be more beneficial for industrialized production and the consecutive production in modern times.
Detailed description of the invention
Mineral element extracted amount such as following table under different condition in the inventive method:
Embodiment 1:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake moving into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), wherein u was enzyme activity unit, by magnetic stirrer 1.5 hours.
4. adding 2mL volume ratio is 1:1 glacial acetic acid solution (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 30 DEG C, ultrasonic extraction 5min under 50MHz, take the supernatant after extraction, to the filtering residue after extracting (in the same terms that is 30 DEG C, ultrasonic extraction 5min under 50MHz) repeatedly extract, ultrasound wave (in the same terms that is 30 DEG C, ultrasonic extraction 5min under 50MHz) extracts three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content obtaining calcium is 1.522mg/g, and the content of ferrum is 0.0045mg/g, and the content of zinc is 0.0102mg/g.
Embodiment 2:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min;
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), by magnetic stirrer 1 hour.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 30 DEG C, ultrasonic extraction 10min under 50MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content of calcium is 1.543mg/g, and the content of ferrum is 0.0049mg/g, and the content of zinc is 0.0104mg/g.
Embodiment 3:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), with magnetic stirrer 1-2 hour.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 30 DEG C, ultrasonic extraction 15min under 50MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content of calcium is 1.511mg/g, and the content of ferrum is 0.0051mg/g, and the content of zinc is 0.0107mg/g.
Embodiment 4:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), with magnetic stirrer 1-2 hour.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 30 DEG C, ultrasonic extraction 20min under 50MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content of calcium is 1.504mg/g, and the content of ferrum is 0.0055mg/g, and the content of zinc is 0.0107mg/g.
Embodiment 5:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), by magnetic stirrer 2 hours.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 30 DEG C, ultrasonic extraction 25min under 50MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content of calcium is 1.534mg/g, and the content of ferrum is 0.0056mg/g, and the content of zinc is 0.0106mg/g.
Embodiment 6:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), by magnetic stirrer 1.5 hours.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 50 DEG C, ultrasonic extraction 5min under 80MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content of calcium is 1.538mg/g, and the content of ferrum is 0.0054mg/g, and the content of zinc is 0.0115mg/g.
Embodiment 7:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), by magnetic stirrer 1 hour.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 50 DEG C, ultrasonic extraction 10min under 80MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content of calcium is 1.571mg/g, and the content of ferrum is 0.0062mg/g, and the content of zinc is 0.0119mg/g.
Embodiment 8:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), by magnetic stirrer 1 hour.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 50 DEG C, ultrasonic extraction 15min under 80MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content of calcium is 1.563mg/g, and the content of ferrum is 0.0060mg/g, and the content of zinc is 0.0115mg/g.
Embodiment 9:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), by magnetic stirrer 2 hours.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 50 DEG C, ultrasonic extraction 20min under 80MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content of calcium is 1.556mg/g, and the content of ferrum is 0.0057mg/g, and the content of zinc is 0.0116mg/g.
Embodiment 10:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), by magnetic stirrer 1 hour.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 50 DEG C, ultrasonic extraction 25min under 80MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content of calcium is 1.560mg/g, and the content of ferrum is 0.0056mg/g, and the content of zinc is 0.0115mg/g.
Embodiment 11:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), by magnetic stirrer 2 hours.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 50 DEG C, ultrasonic extraction 5min under 100MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content of calcium is 1.558mg/g, and the content of ferrum is 0.0059mg/g, and the content of zinc is 0.0112mg/g.
Embodiment 12:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), by magnetic stirrer 1.5 hours.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 50 DEG C, ultrasonic extraction 10min under 100MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content of calcium is 1.565mg/g, and the content of ferrum is 0.0055mg/g, and the content of zinc is 0.0114mg/g.
Embodiment 13:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), by magnetic stirrer 1 hour.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 50 DEG C, ultrasonic extraction 15min under 100MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content of calcium is 1.561mg/g, and the content of ferrum is 1.0058mg/g, and the content of zinc is 0.0116mg/g.
Embodiment 14:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), by magnetic stirrer 2 hours.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 50 DEG C, ultrasonic extraction 20min under 100MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content of calcium is 1.564mg/g, and the content of ferrum is 0.0059mg/g, and the content of zinc is 0.0115mg/g.
Embodiment 15:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), with magnetic stirrer 1-2 hour.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 50 DEG C, ultrasonic extraction 25min under 100MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content of calcium is 1.563mg/g, and the content of ferrum is 0.0057mg/g, and the content of zinc is 0.0117mg/g.
Embodiment 16:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), by magnetic stirrer 1 hour.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 70 DEG C, ultrasonic extraction 5min under 100MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content of calcium is 1.549mg/g, and the content of ferrum is 0.0054mg/g, and the content of zinc is 0.0112mg/g.
Embodiment 17:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), by magnetic stirrer 2 hours.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 70 DEG C, ultrasonic extraction 10min under 100MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content of calcium is 1.547mg/g, and the content of ferrum is 0.0055mg/g, and the content of zinc is 0.0117mg/g.
Embodiment 18:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), by magnetic stirrer 1 hour.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 70 DEG C, ultrasonic extraction 15min under 100MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content of calcium is 1.551mg/g, and the content of ferrum is 0.0055mg/g, and the content of zinc is 0.0122mg/g.
Embodiment 19:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), by magnetic stirrer 1.5 hours.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 70 DEG C, ultrasonic extraction 20min under 100MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
7. being dried by the liquid after concentration, the content of calcium is 1.558mg/g, and the content of ferrum is 0.0057mg/g, and the content of zinc is 0.0111mg/g.
Embodiment 20:
1. Folium Lycii cleaned, at 50-60 DEG C, dry 8-12h, grind and cross 60-80 mesh sieve.
2. accurately weigh the 1g powder sieved in beaker, add appropriate No. 6 light gasoline 6mL and stir sucking filtration after 20min.
3. filter cake is moved into the deionized water adding 10mL in beaker, instills two cellulase (130-150u/ml), by magnetic stirrer 2 hours.
4. adding 2mL volume ratio is 1:1 glacial acetic acid (glacial acetic acid volumetric concentration 50%), uses magnetic stirrer half an hour.
5. at 70 DEG C, ultrasonic extraction 25min under 100MHz, take the supernatant after extraction, filtering residue after extracting is extracted repeatedly, ultrasonic extraction three times, will supernatant after three ultrasonic extraction merge after carry out sucking filtration, merging filtrate with deionized water constant volume to 50mL.
6. in the filtrate that constant volume is good, add 200mL dehydrated alcohol, stand 2h and fully precipitate, be centrifuged and obtain supernatant, 1/5 to original volume is steamed in supernatant rotation.
Being dried by liquid after concentration, the content of calcium is 1.559mg/g, and the content of ferrum is 0.0057mg/g, and the content of zinc is 0.0113mg/g.
Claims (4)
1. the method for an enzymolysis and extraction Folium Lycii mineral element, it is characterised in that comprise the steps:
(1) raw material: Folium Lycii is dried;
(2) pulverize: the Folium Lycii after drying is pulverized;
(3) screening: the Folium Lycii powder after pulverizing is crossed 60-80 mesh sieve;
(4) defat: add No. 6 light gasoline in the powder obtained and soak, then stir, then sucking filtration drying, obtain removing the Folium Lycii powder of fat;
(5) enzymolysis: obtain the Folium Lycii powder arrived, add deionized water according to 1g Folium Lycii powder/10-20mL, adds cellulase according still further to 130-150u/mL, stirs 1-2 hour;
(6) acidifying: the sample after enzymolysis is added according to 1g sample/1.5-2mL glacial acetic acid or glacial acetic acid solution, stirs 0.5-1 hour;
(7) ultrasonic extraction: at 30-70 DEG C, ultrasonic extraction 5-25min when 50-100MHz, take the supernatant after ultrasonic Treatment, to precipitate according still further to condition ultrasonic extraction same as before, take the supernatant after ultrasonic Treatment, to precipitate according still further to condition ultrasonic extraction same as before, take the supernatant after ultrasonic Treatment, finally merge the supernatant extracted three times;
(8) filter: the extracting solution sucking filtration that will obtain, discard filtering residue;
(9) concentration: carry out the concentrating under reduced pressure 1/3-1/5 to original volume with the vacuum distillation apparatus extracting solution to obtaining;
(10) dry: by the liquid drying after concentration to mineral element extract.
2. the method for enzymolysis and extraction Folium Lycii mineral element as claimed in claim 1, it is characterised in that: step (1) is dried and refers to 50-60 DEG C of drying 8-12h in blast drier.
3. the method for enzymolysis and extraction Folium Lycii mineral element as claimed in claim 1, it is characterised in that: step (4) controls No. 6 light gasoline liquid levels and did not have powder 1-1.5cm, control mixing time 0.1-2 hour.
4. the method for enzymolysis and extraction Folium Lycii mineral element as claimed in claim 1, it is characterised in that: step (10) is dried and refers to drying at 50-60 DEG C.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106616330A (en) * | 2017-02-03 | 2017-05-10 | 宁夏林业研究院股份有限公司 | Method for improving quality of noodles by adding folium lycii extract |
CN106666319A (en) * | 2017-02-03 | 2017-05-17 | 宁夏林业研究院股份有限公司 | Lycium Chinense miller leaf extract effervescent granule and preparation method thereof |
CN106723049A (en) * | 2017-02-03 | 2017-05-31 | 宁夏林业研究院股份有限公司 | A kind of method that HTHP extracts folium lycii mineral element |
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CN104833560A (en) * | 2015-04-27 | 2015-08-12 | 宁夏森淼种业生物工程有限公司 | Quickly-shearing nondestructive method for extracting mineral elements from wolfberry leaf |
CN104839738A (en) * | 2015-04-27 | 2015-08-19 | 宁夏森淼种业生物工程有限公司 | Method for high-efficiency extraction of mineral elements in wolfberry leaves through ultrasonic process |
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104833560A (en) * | 2015-04-27 | 2015-08-12 | 宁夏森淼种业生物工程有限公司 | Quickly-shearing nondestructive method for extracting mineral elements from wolfberry leaf |
CN104839738A (en) * | 2015-04-27 | 2015-08-19 | 宁夏森淼种业生物工程有限公司 | Method for high-efficiency extraction of mineral elements in wolfberry leaves through ultrasonic process |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106616330A (en) * | 2017-02-03 | 2017-05-10 | 宁夏林业研究院股份有限公司 | Method for improving quality of noodles by adding folium lycii extract |
CN106666319A (en) * | 2017-02-03 | 2017-05-17 | 宁夏林业研究院股份有限公司 | Lycium Chinense miller leaf extract effervescent granule and preparation method thereof |
CN106723049A (en) * | 2017-02-03 | 2017-05-31 | 宁夏林业研究院股份有限公司 | A kind of method that HTHP extracts folium lycii mineral element |
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